Artificial yarn and method of preparing the same



Patented g 35 y y I I UNIT D STATES PATENT OFFICE YVAR'N AND ME'rn'on onPRE- lv PARING THE SAME' V I Camille Dreyfus, New York, N. ,Y., andWilliam Y Whitehead; Cumberland; .MdaFassignors to Celanese Corporationof America,;a corpora?- tiontof De lawarev No Drawing: Application June16,, 1928, i ;Serial No. 286,070 I 1 5Claims. (01.18-54) a I Thisinvention relates to the preparation of formate, cellulose-propionateand cellulose butyartificial yarns andparticularly' yarns-made of ratewhile examples of cellulose ethers are methyl Containing organicderivativesfof cellulose cellulose, ethyl cellulose and ,benzylcellulose. Such as iq l e acetate from solutions contain- However,because'of the superior results obtained 5 ingthe same. by its use, weprefer cellulose acetate whichrrnay E 6 Anobject of ouriinventionis toprepare yarns or may not be solublep m p c fically containing organicderivativesjofrcellulose, parwe prefer to use. an acetime solublecellulose aceticularly cellulose acetate, which yarns are'eastatehav'inganacetylwalue of 52.5% to 56%; and c J ilywettedj bywater, whereby fabrid of preferably 5 l x5%', but thisinvention is not limited 10 the same.may be readily scoured, dyed and/or 0 the used u cellulose acetategivean other desired finishing treatment. h l we d n t lim t u selves toa spoific A further objectrof our.inventionis toprepare o t Solvent o b usedr c we artificial yarns containing organic derivatives have'found th tacetone ar b of'cellulos'e such as cellulose acetate, which yarns 's s'tj I l The r la ve 1011:?913 16 may besubjectedtofurthertextilelo er tgs b tile substancexadded tether-spinning solution as knitting orweavin'g'without the "additien f may beanypsuitable substance that. ismiscible c lubricants, o 'with the-additionsjofilesslubricants withthecvqlatile Solvent d in e ar n xi hi than have heretoforei'been used;I Spinning 559111121011, a which s 9 Q l b i A furtherobjectfof ourinvention is td'piii re t is cap i ii ns l ithit e 20 artificial" yarnscontaining organic" derivatives organiffderivatives 9 19 0 w W- 2 5jects of ouninventionswillappear fromthe jfol ducedfromsuchsolutionsfmay be more, readily of f cellulose and" particularlycellulose acetate, paring I H which'yarns produce. lesssnarlinglintextile:operhave found that r ativ -Volat e al- 'ations and which do notbreak as readily in looms 9011015 are n t y Suited 9 hi r s W as prior,artificialiyarnsof mistyped-[Other obe found? particularly ithat ht s sethylene glycol or diethylene glycol give eminently lowingjdetailed' desipti p v satisfactoryresults," Likewise we havefound'thatci I In thepi'paratidh' ofartifi ia1 f m on glycerol and diacetone alcohol are veryus'eful in i garlic. derivatives. of cellulose such; as celluloseithisvpmcess" A n cont-aming i acetate,lthemostZgenerallyusedniethod'involves @1 9 groups ehia e ke on c m w the spinningofsolutions of the sarne iniayolatile s fl v u e F h mo lithe-rs 9 m .solvent into an. evaporative atmosphere; asinthe "relatively Q t F i J Such.as the a dry spinning procession-into a'precipitating bath of glycol d fiof which h m j as in the wet spinning process. M .ethylgther ofethylepe 9 mentioned we have found the surprisingsfactthatfia aresuitable foruse n th1srnvent1on; 'I 'he term v v ,atively: nonvolatilesubstance is added to the freIQftIVEIY non'vqlame t i q as us-ed m fstunningsolution containing the organic derivalispeclfica'twn and m the019111.115 1s p d tive sofi cellulose, which" substance soluble in iiggq' i igg g igs ggg 52 33 632 ggz water or any other scouring ncy,yarns. proorganic derivatiyesyinlfaivolatfle solvent ov ingthesesubstances is evaporated at atemper; I 3 g? fgi gifis giig gfifii zg gfi ll l ailre which is suificient to volatilize the volatile 'tionsis-notgenerally'required 8 open -9 thgse substance mmamlargaily I f dt1l1z ed, and are present in the y arn to.1rnpa r the: o 11, 8100018,1106 W]. 0111 lIlVell. 1011, prepare c i 14- 'amsolutioncontainingthe. organic derivatives of The amountbtrelativgly nonvolatfle subs e cellulosecin a volatile-solvent, to. which" solution ais soluble in wa t g aa t th vis: also added a" relativelynon-volatilesubstance spinning solution, may be varied within wide lur'i t 'WhlCh'is. miscible "Wlth "the? solution, and which t d 'ndingpp'onthe natureofithe substan ces' m y readlly removed from theyam used andtheresultsrequired? Generallywe have ab q fq e f m' QY y scouring n foundthat'if the organicderivatives of cellulose M ter or anyo a escouringzagency; are dissolved in solventmixtures containing from;

Theorganic derivative of cellulose used for l to 30% of the relativelynon-volatile substance, making the yarn may be any suitable organicexcellent results are obtained. "Theternfierature' esters or ethersof-cellulosei Examples of organic *of the-spinningmay also be 'vari edin'a ccordance "55 Testers of-cllulose are cellulose-acetate,'-cellmosewith-the -natureofth'e- -volatile solventfused'filie accordancewith ourprocess is self lubricated and therefore further lubrication for textileoperations nature of the relatively non-volatile substances used, andthe relative proportion of non-volatile substances to volatile solvent.

Yarns produced by the dry spinning of solutions of organic derivativesas above described,

retain a large percentage of. the relatively nonvolatile substancesadded, and sinee these substances are soluble in water, the yarn or thefabric from'which the. yarn is, formed may be readilyi" wetted bywater.- This is of great, advantage in such as.winding,twisting,knitting and 'weaving'is not absolutely required with these'yarns.Moreover, these yarns produce less snarling when twisted and lessbreaking in the loom thanprior yarns, which is obviously a greatadvantage.

Although the yarns made in accordance with our- 'invention-are weakerthan prior yarns while .they'still contain :the relatively non-volatilesub-. stances that have been addedto the spinning solutionj theyare of'sumcient strength towithstand the strains to whichfthey are subjectedin ordinarytextile operations. However, after they are thoroughlyscoured, which scouring may bedone onthe yarns priorto making themintofabric, but

which is; preferably done after they areformed into fabrics, theyarnshave strength atleast equal to that of yarns formed fromsolutionsnotcontaining these relatively non-volatile substances, and inmany. cases they are'actually stronger.

Inorder', furtherto illustrate our inventionibut without in anywaylimiting ourselves thereby, the

following specific examples are given.

g Exemplar We take. a cellulose acetate having an acetyl .value of 54.5%andaviscosity of 20 as determined on an Oswald Viscosimeter with. asolution'ioffi grams of cellulose" acetateand- IOOgrams of acetone, thevisco'sity of glycerol being called 100.) cellulose acetateznormally has'arnoisture .content. of 5% and maybe used directly in our process.However, if desired,. the cellulose acetate may be placed in a vacumndrier where it is dried at an'elevated temperature under a vacuum of 25.f of mercury.I (i e. 5"" of mercury absolute pressure) untilitsmoisture content is reduced below 1%. The cellulose acetate is thendissolved in a mixture containing from 1to.5% of diethylene glycol andfrom 99. to 95% of acetone, in

amounts sufficient to. form a solution containing substantially 25%01":celluloseacetate. The solution 'isthen'filtered, andspun in a dryspinning machine wherein thesolvent is evaporated'off at atemperature'ofz55 to (3., the. thread thus formed:'being gathered up andwound or reeled.

. 'Ilheyarhi-prddnced,in manner displays a remarkable increase inability to being. wetted by wate This is indicated by tl efactj that ifa fabric made of this yam'j s placed-on the surface r water, it sinksinl5j seconds, whereas fabric made from yarn which-hasbeen formed fromsolutions not containing the diethlene glycol does 'lnot sink in wateruntil after 60. seconds.- The yarn is' self lubricated and may besubjected to .textilefoperations, without further lubrication. :A erihvarna i cbu e i w crto r move: th

diethylene. glycolywhich present therein and I then dried, the yarnshows an ability to regain moisture of about 8% of itsweight as againstabout 5% of its weight for a yarn formed in accordance with the priorpractices. When this yarn is highly twisted and made; up j into crepe ofis level and otherwise satisfactory,a result which was not obtainable bylthe use of yarnmade by priorprocesses.

ErampleIl V Thecelluloseacetate such as described in Exhample I isdissolvedin a solvent mixture containing l' to 10% of diacetone' alcoholand 99 to 90% of fabricssuch as crepe .marocainJthe dyeing thereiacetone-respectively, and preferably a solvent mix-,

-ture containing substantially 5% of diacetone alycqhcl and 95% ofacetone. The concentration of the solution is such that preferably'itcontains about'25% of the cellulose acetate. I The cellulose acetateand'the solventare mixed with thorough agitation for about 5 to 6 hourstoobtain a sufficiently homogeneous solution, The solution isthenfiltered and spun in a dry spinning machine :25 Y

wherein the solvent is evaporated offatav temperature of 55 to C.,andpreferably atsuch rate'that meters of filament or yarn are formedpermin'ute. The thread or yarn thus formed isgathered up and wound orreeled. The

yarn produced in this manner contains diacetone alcohol whichhas notevaporated off at thespinning temperature, and displays all thedesirable characteristics. of readiness 'to wetting, 'ease of -dyeingand selfilubrioating'properties as the yarn made in, accordance withEx'ample I. This yarn afterjwashing in five changes of water'a't- 40 C.has a dry tenacity of 1.4. grams per denier 'as against a tenacity of1.3 foryarnfprepared from solutions not containing the diacetonealcohol.

' It is ,to" be. understood that the foregoing: de-

taileddescription isgiven merely by way, of illustration and that manyvariations may be made therein'without departing from the spirit of thisinvention.

' v Having described our inventionwhatwe claim and desire'to secure: byLetters Patentis:

. 1. The method of' producing yarns containing organic 'derivatives ofcellulose which com- 'prises spinning a solution of the organicderivatives of cellulose: ina mixture containing a. vola- "tile' solventtherefor and a relativelynon-volatile polyhydric alcohol that isanon-solvent for the organic derivatives of cellulose and is soluble inwater. t t

2. Thej methodof producting yarns containing organicderivatives ofcellulose which "comprises dry'spinning a solution of the organicderivatives of cellulosein'a mixture containing a volatile solventtherefor and a relatively nonvolatile polyhydric alcohol that is anon-solvent for-the organic derivatives of cellulose and is soluble inwater. v

3. The method of producing yarns containing cellulose acetate whichcomprises dry spinning a solution of the cellulose acetate in a mixtureatively non-volatile polyhydric alcohol that is a non-solvent for thecellulose acetate and is soluble in water;

.4. The method of producing yarns containing cellulosejacetatecomprising dry spinning a solution of the cellulose acetate in amixturecontaining acetone and glycerol. l

5. Ina method of producing yarns containing cellulose acetate,-the stepof dry spinning a so- 3 containing a volatile solvent therefor andarelalution of cellulose acetate in acetone which so cellulose acetate,the step of dry spinning a solution of cellulose acetate in acetonewhich solution also contains diethylene glycol.

7. Yarn containing organic derivatives of cellulose and a relativelynon-volatile polyhydric alcohol'that is a non-solventfor the organicderiv'atives of cellulose and is soluble in water.

8. Yarn containing cellulose acetate and a relatively non-volatilepolyhydric alcohol thatis a non-solvent for the cellulose acetate and issoluble in water. p

9. Yarn containing cellulose acetate and a glycol.

l0. Yarncontaining cellulose acetate and diethylene glycol. I V

11. The method (is producing yarns contain ing organic derivatives ofcellulose, which comprises spinning a solution of the organic deriva,tive of cellulose ina medium containing a vola- 'tile solvent thereforand a proportion of from 1-30% of a relatively non-volatile polyhydricalcohol that is a non-solvent for the organic de- 12. The method ofproducing yarns containing cellulose acetate, whichcomprises drys'pinningj; a solution of cellulose acetate in a medium'con taining avolatile solvent therefor 'andla prof v portion of from 1-30% of arelatively non-V012,;- 5 tile polyhydric alcohol that is anon-solve'ntfor I the cellulose acetate and issoluble in water. 1';

13. The method of producing yarns contain ing cellulose acetate,comprising dry-spinning a solution of cellulose acetate in a medium'con10 f taining acetone and a proportion of from 1-30%; of a glycol. 14.The method of producing yarns containing cellulose acetate, comprisingdry-spinning a solution of cellulose acetate in amediumicon tainingacetone and a proportion of from 1-30% of diethylene glycol. j

g 15. The method of producing yarns contain-' ing cellulose acetate,comprising dry-spinning a solution of cellulose acetate in a mediumcontain- 0 ing acetone and a proportion of from 1-30% of glycerol.

CAMILLE DREYFUS;

WILLIAM WI-HTEHEAD. g

